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Designation: D 3103 – 99

Standard Test Method for


Thermal Insulation Quality of Packages1
This standard is issued under the fixed designation D 3103; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope
1.1 This test method covers the determination of the thermal
insulation quality of a package and its enclosed packaging from
temperature differentials between the packaged item and the
outside environment. It is suitable for testing packages with
and without various internal refrigerants and with or without
interior packaging. Representative test conditions covered are
indicated by Fig. 1 and Fig. 2. Depending upon the type of
insulation material used, a water-vaporproof barrier might be
used just inside the exterior packages of Fig. 1.
a—Containers Having Usable Inside Volume of 1 ft3(0.03 m3) or Less.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in 5.2.3 and 9.2.2.
2. Referenced Documents
2.1 ASTM Standards:
D 996 Terminology of Packaging and Distribution Environ-
ments2
b—Containers Having a Usable Volume of More Than 1 ft3(0.03 m3)
D 4332 Practice for Conditioning Containers, Packages, or
FIG. 1 Thermally Insulated Packages with Sensors Positioned
Packaging Components for Testing2
3. Terminology 3.2.6 interior package—a package (often of corrugated
3.1 Definitions—General definitions for packaging and dis- fiberboard) located within another.
tribution environments are found in Terminology D 996. 3.2.7 thermal conductivity, homogeneous material—the
3.2 Definitions of Terms Specific to This Standard: rate of heat flow, under steady conditions through unit area, per
3.2.1 draft-free atmosphere—a relatively stationary atmo- unit temperature gradient in the direction perpendicular to the
sphere where the test specimens are remote from air currents. area.
3.2.2 eutectic system, n—a mixture or compound in which
4. Significance and Use
pure solid phases changes occur at a well-defined specific
temperature. 4.1 Certain items, such as biological materials, pharmaceu-
3.2.3 exterior atmosphere—the atmosphere in contact or ticals, industrial adhesives, gyroscopes, blood, and some foods,
near the exterior surface of a package. must be shipped inside temperature-controlled packages. Fac-
3.2.4 exterior package—the outermost container of a pack- tors affecting the rate of heat transfer of the package include the
age. moisture content of the different package components and the
3.2.5 interior atmosphere—the atmosphere in contact or thickness, continuity, density, position, and uniformity of the
near the packaged item. insulation.
4.2 Because of the variety of factors affecting the perfor-
mance of a thermally insulated package, testing should be
1
This test method is under the jurisdiction of ASTM Committee D-10 on conducted with the actual package whenever possible. When
Packaging and is the direct responsibility of Subcommittee D10.23 on Natural simulated packages are used, special care must be exercised so
Environment Test Methods.
Current edition approved Oct. 10, 1999. Published December 1999. Originally
that the simulated payload and coolant of the model will be as
published as D 3103 – 72. Last previous edition D 3103 – 92. close as possible to the actual materials in temperature and
2
Annual Book of ASTM Standards, Vol 15.09. other relevant physical properties.

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

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D 3103
tion of the device shall be 0.1°C or greater. Accuracy over the
range tested should be 6 1°C. The printer or associated
computer datafile shall be activated by a voltage from an
insulated pair of copper-constantan or other suitable wires 30
AWG B&S gage (0.255 mm) or less in diameter (not including
the thickness of insulation). The recorder and chart shall have
a capability that extends beyond the temperature values en-
countered in the test.
5.3.2 Thermistor-Recorder—A thermistor sensor may be
used, instead of a thermocouple, for sensing interior tempera-
tures of the package. The thermistor may be attached to
recording equipment, as described in 5.3.1, with supplementary
electrical circuitry as needed, or it may be a wireless, battery
operated, computer programmable unit that stores digital
temperature readings at specified time intervals. Programming
and data downloading of the units is done through a suitable
computer interface with appropriate software. Accuracy over
the range tested should be 6 1°C with resolution to 0.1°C.
Response time over range should be determined prior to use
and suitable for the reading interval of the test.
6. Sampling
6.1 Experimental package designs shall be made in accor-
dance with the specifications and methods that will be used
FIG. 2 Liquid Nitrogen Refrigerator during actual production. When possible, choose the test
packages by random sampling.
5. Test Conditions and Apparatus
5.1 Temperature of Exterior Atmosphere— Draft-free envi- 7. Test Specimens
ronments large enough to accommodate the packages, but not 7.1 A single test specimen shall consist of a package
necessarily the recorder, are required. Usual evaluation of the enclosing the actual item or a dummy load simulating the item.
packaging materials will involve simple refrigerated or ambi- The package shall be closed, taped, or sealed in the same
ent exterior atmospheric conditions. These may be established manner as will be used for actual shipment.
as 4 6 2°C (39 6 4°F), 37.8 6 2°C (100 6 4°F), and 23 6 2°C 7.2 The mass, configuration, and location of refrigerant, if
(736 4°F). Additionally, other temperature extremes or cycles used, must be the same in each pack.
between various temperatures expected during shipment might 7.3 For development or screening evaluation of the overall
be used as an exterior atmosphere. insulation effectiveness of the container and insulation mate-
5.2 Temperature of Interior Atmosphere of Package—When rial, the interior cavity and package wall thickness shall be kept
no refrigerant is used, interior package temperature may serve constant (for example, a 12 by 12 by 12-in. (305 by 305 by
as a measure of the thermal insulation quality of the package. 305-mm) interior cavity surrounded by a 1-in. (25-mm) thick-
If it is desired to control the interior temperature of the ness of insulation and a 14 by 14 by 14-in. (356 by 356 by
atmosphere, use one of the following: 356-mm) container. Test a minimum of three such packages at
5.2.1 Refrigerant Gel, Water Ice, or Other Refrigerant each exposure listed in 5.1 to obtain an average result and
Source, for internal temperatures above 0°C (32°F), range of performance.
5.2.2 Solid Carbon Dioxide CO 2(Dry Ice or Euctectic 7.4 When testing packages having known or previously
Systems), wrapped as used in shipments for maintaining established performance data, a minimum of three identical
internal temperatures down to − 73°C (−108.4°F), or samples shall be tested to determine reproducibility and
5.2.3 Liquid Nitrogen, for temperatures to − 195°C repeatability.
(−319°F).
8. Conditioning
NOTE 1—Caution: Gaseous CO2 and nitrogen are colorless, odorless,
and noncombustible. In well-ventilated uses they present few problems, 8.1 Condition materials in accordance with Practice D 4332
but evaporation or sublimation in airtight enclosures for prolonged periods or for 24 h at the conditions expected during actual production
(for example, 12 h) can produce sprung doors and asphyxiation of packing.
operating personnel. Usually these refrigerants can be used if provisions
are made to evacuate the built-up gas periodically. 9. Procedures
5.3 Temperature Indicators: 9.1 Packages Enclosing Solid Refrigerants:
5.3.1 Multi-Channel Recorder with Thermocouples—The 9.1.1 Verify the calibration of the temperature-monitoring
recording capability should be as a datalog by thermocouple equipment per manufacturer’s directions against an NIS trace-
number with date and time of reading, that can be presented in able standard suitable for the ranges being measured. Battery-
a continuous graph form as a secondary presentation. Resolu- operated thermistors recorders with or without external probes,

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D 3103
should be calibrated by the manufacturer and a certificate of insulated carton, place the cover on the package with the sensor
NIS traceability of accuracy provided. wires arranged so that the least possible heat transfer occurs
9.1.2 Place the contents in the conditioned package accord- through the joint.
ing to the specific configuration to be tested. 9.1.6 Tape or otherwise secure the cover to the package in
9.1.3 Insert the sensors in the package so that they are in the normal manner.
contact with the item(s) as follows: 9.1.7 Place the package in the test environment on a wooden
9.1.3.1 For packages having an inside volume of 1 ft 3 or platform or shelf in such a manner that no part of the package
less and a single open cavity for both ice and product, place contacts the chamber walls or floor. If more than one package
one sensor at or near the diagonally opposite corners of the is tested at one time, they shall be separated from each other by
item as shown in Fig. 1a. Additionally, the sensors and at least at least 6 in. (152 mm). Mark the chart with date and time and
1⁄2 in. (13 mm) of wire immediately behind them should be in
start the recorder.
contact with the item. Wrapping the wires around the item, if 9.1.7.1 The orientation of the carton should be the same as
practical, is advantageous to minimize heat flow from the that experienced in shipping. For small cartons where various
outside. orientations occur during shipping, all orientations should be
9.1.3.2 For packages designed with interior walls separating screened and tested, as the orientation affects the interior
product and refrigerant, more thermocouples may be needed to temperature profile. If more than one carton is shipped at a
adequately monitor temperatures. Again, porting through a time, duplicate the usual configuration of the units during
wall directly into the product cavity is recommended. The port shipping in the test, as the added insulation value of adjacent
should be kept as small as possible and sealed after insertion of cartons affects the time/temperature profile of the carton as
thermocouples to prevent leaking air. well as location of coldest and warmest spots.
NOTE 2—It is desirable to use wireless data recorders, if possible, on 9.1.8 If data is collected in digital format, the recorder
smaller units to minimize temperature leaks at the thermocouple insertion should be set to record temperatures not longer than every 30
site. If thermocouples are used, a small port can be opened through the to 60 min in screening tests. Intervals as short as 5 min may be
wall of the carton as far away from the ice as possible, the thermocouples needed for thin-wall containers exposed to low exterior air
inserted into the carton, and the port sealed to prevent leaking of air. Do temperatures. Once a temperature profile has been established,
not place battery operated recorders in packages containing dry ice as the recording intervals can be extended to every 3 h, depending on
units will be damaged and nonfunctional at these temperatures. Units with
remote probes may be placed outside the carton where the battery and
the duration of the test and the rate of internal temperature
microchip will not be exposed to dry ice conditions. change. Continue to collect data until the interior temperatures
are above the maximum or below the minimum temperatures
9.1.3.3 For packages having usable inside volume of more dictated by the product, or until the total test time has elapsed.
than 1 ft3, a screening test using a minimum of ten thermo- If the data can be reviewed on an exterior monitor, end the test
couples to determine the locations of the warmest and coldest when the desired limit is reached. If using micro-chip based
spots is recommended. The larger the usable capacity, the more battery operated recorders without exterior monitoring, end the
thermocouples may be needed to adequately screen and test the test when the total elapsed time limit is reached.
package. Packages with interior walls separating product and
refrigerant may require testing at extreme temperatures above NOTE 3—Larger capacity cartons show a slower rate of temperature
change than small cartons. Temperature reading intervals should be
or below those specified in 5.1 to fix locations of hot and cold
adjusted to the rate of change, that is, shorter for small packages with
spots. Every interior configuration, including quantity and lower insulation values and longer for larger packages with higher
placement of both ice and product should be screened, as insulation values.
changes to either element will alter the interior temperature
profile of the package. Once warmest and coldest locations are 9.1.9 Check the calibration of the temperature-monitoring
identified, the number of thermocouples can be adjusted equipment at the end of the test.
upward or downward, depending on the reproducibility of the 9.1.10 Mark the date and hour of the start and end of the
warm and cold locations. testing on the chart or digital data record.
9.1.4 Place a weighed and measured quantity of refrigerant 9.2 Containers with Liquid Nitrogen Refrigerant (Fig. 2):
in the package. When water ice or refrigerant gel are used, 9.2.1 Detach the necessary sensor wires from the tempera-
measure and record their temperature at the start of the test. Do ture recorder, calibrate, and place the sensing end(s) within the
this by securely taping a sensor to the outside of the refrigerant container adjacent to the contents.
container or by inserting a sensor into the water prior to 9.2.2 Condition the container and contents by immersing
freezing. them in liquid nitrogen for the length of time specified by the
9.1.4.1 The quantity of refrigerant or eutectic system may manufacturer, or by another recommended method.
be varied. However, when materials and designs of similar N OTE 4—Caution: The temperature of liquid nitrogen is
inside dimensions are being evaluated, the quantity by mass, about − 195°C (−319°F). Therefore, when liquid nitrogen is used as the
configuration, and total surface area must be constant for the cooling agent, extreme care must be used during purging to maintain a
series for accurate evaluation of performance. When crushed or nitrogen atmosphere adjacent to surfaces having a temperature near that of
chopped dry ice is used, the fragments should be of the same liquid nitrogen. This is necessary to prevent oxygen condensation and the
related explosive fire danger.
general size for each package tested and should be free of dry
ice dust. 9.2.3 With the contents in the conditioned container, add the
9.1.5 If wires are not ported through the wall of the liquid nitrogen as recommended by the container manufacturer.

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D 3103
9.2.4 Attach the cap or closure to the container with the 10.1.7 Number of hours recorded on the chart or digital data
sensor wire or wires extending between the closure and record by each sensor from the start of the test to the point
container in such a manner that the least possible nitrogen where the temperature starts to exceed the maximum or
leakage occurs. minimum temperature established for the test.
9.2.5 Attach the ends of the sensor wires to the recorder and 10.1.8 Quantity, temperature, and state (if pertinent) of
proceed as in 9.1.7. refrigerant remaining at the end of the test, or the test duration
9.2.6 Allow the recorder to run until the indicated tempera- has been reached.
tures are above the maximum established for the particular test. 10.1.9 Description of the physical state of the contents at the
9.2.7 Check the calibration of the temperature-monitoring end of the test.
equipment and record the date and hour. 10.1.10 Evaluation of the test with respect to the effective
9.3 Packages Without Refrigerants: storage time in comparison to tests of other packaging mate-
9.3.1 When packages are tested without refrigerants, the rials or other designs.
thermal insulation quality is determined by observing the 10.1.11 A statement that all tests were made in accordance
temperature change between the interior atmosphere or product with this test method.
and the controlled atmosphere outside the package.
9.3.2 Calibrate the temperature-monitoring equipment. 11. Precision and Bias
9.3.3 If the package (with or without interior packaging), is 11.1 Precision—The precision of this test method has been
to be tested empty, place at least one sensor on the inside determined by an interlaboratory study.
surface of the package, and at least one additional sensor near 11.1.1 Repeatability—When an analysis is conducted on the
the center of the package. times in hours to reach a critical temperature, the within-
9.3.4 If the package is to be tested with the product, embed laboratory standard deviation is typically about 4 % of the
at least two sensors in or in contact with the product, or as mean. When a lognormal analysis is conducted on the natural
many sensors as are needed to test the entire interior. logarithms of the time in hours, the typical within-laboratory
9.3.5 Suspend one sensor in the controlled atmosphere standard deviation is 0.04. These values may vary depending
outside and in close proximity of the package(s) to serve as a on the package or container being tested and the capabilities of
check against the usual recording controls of the environmental each laboratory.
chamber. 11.1.2 Reproducibility—When an analysis is conducted on
the times in hours to reach a critical temperature, the between-
10. Report laboratory standard deviation is typically about 10 % of the
10.1 Report the following information: mean. Then a lognormal analysis is conducted on the natural
10.1.1 Dimensions of the package under test, its structural logarithms of the times in hours, the typical between-
specifications, the materials of construction, the name of laboratory standard deviation is about 0.1. These values may
manufacturer, and the method of securing the lid. vary depending on the package or container being tested and
10.1.2 Description of item(s) and secondary packaging the capabilities of each laboratory.
materials. 11.2 Bias—It is not possible to specify the bias of this test
10.1.3 Type, quantity, and location of refrigerant and de- method as no accepted reference material or method is avail-
vices within the package (in the case of water ice and able.3
refrigerant gel, record the initial ice and gel temperatures).
10.1.4 Type of temperature recording system used, (if a 12. Keywords
thermocouple system was used, indicate the location of ther- 12.1 heat transfer of packages; thermal insulation; tempera-
mocouple leads and junctions within the package). ture controlled packages
10.1.5 Method of conditioning package and contents prior
to test.
10.1.6 Temperature and relative humidity of the test envi- 3
Supporting data have been filed at ASTM Headquarters and may be obtained by
ronment. requesting Research Report RR: D10–1012.

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